Process for the production of cellulose solutions.



EMILE GRUMIERE, or rams, FRANCE;

raocnss roa mm raonuo'rron' or cE-LLuLosE SOLUTIONS.

Specification of Letters Patent.

Patented Jan. 5, 1909.

Application filed-October 18, 1906. Serial No. 339,459.

. Tooll whom it may concern:

' in Paris, France, have invented certain new and useful Improvements in Processes for the Production of Cellulose Solutions, of which the following is a specification.

The remarkably energetic oxidizing power of ozone which is now obtainable on an in dustrial scale has suggested to the present applicant that cotton or cellulose that has to be dissolved in ammoniacal cupric solution might advantageously be treated with ozone in order to produce the intense oxidizing action which, as the applicant has ascertained, is favorable to the manufacture of artificial silk. e

The researches which the applicant has made in the subject have shown that ozone, by virtue of the particular oxidation that it produces, brings the cotton into a condition in which it not only dissolves with advantageous rapidity in the ammoniacal cupric solution, but also yields a solution of cellulose having body, that is to say a condition essential for the production of satisfactory threads having suitable resistance. Moreover, the applicant has found that the artificial silk prepared-from the solution shows a beautiful white silky appearance.

The invention relates, therefore, to the treatment of cotton or cellulose which is to be used for the manufacture of artificial silk or the like with ozone.

In applying the ozone to the cotton certain substances, among which are alkaline bodies, such as caustic soda, potash, or a mixture thereof, facilitate the penetration of the oxidizingaction throughout the mass of the cotton fibers, thus producing a uniform distribution of the action. In practice the 'cotton may into contact with a solution of soda for ex-.

ample, through which is bubbled for 30 mlnutes or so a current of ozone or of ozonized air produced by any suitable ozonizing apparatus.

The ozonizing of cotton in the presence of I an alkaline solution may be advantageously "carried out in the following'manner: (1) A solution of caustic soda or caustic potash (say 25 cubic centimeters of a solution of soda of 1.4 density 'per liter of water) to make 15 or 20 liters per kilo of cotton to be treated is prepared and into this a current of ozone is passed for some five minutes.

be brought.

nized caustic solution and a current of ozone is passed for about thirty minutes more, the mass being stirred during the operation. (3) The current of ozone is stopped and the whole is boiled for about thirty minutes. The ozone is introduced in both cases in the form of air containing about 0.2 milligrams of ozone per liter of air. The air is introduced at approximately the rate of 72,000 liters per hour. This with the ozone content indicated would give the rate of circulation of the ozone as 14A grams per hour. This quantity of ozone, 14.4 grams is about the quantity which would be furnished by an electric current of 120 watts.

The cotton thus prepared is washed,

dried in the air, and is then ready for the.

ing a high degree of resistance and great elasticity.

In proportion as the ammoniacal cupric solution dissolves the cellulose, the solution becomes impoverished in copper, and in order to control the dissolving action the present invention provides for maintaining the strength of this solution in copper practically constant. For this purpose a certain quantity of free metallic copper 1s added to the ammoniacal cupric solution prepared in the ordinary manner.

When the cotton prepared in the manner aforesaid is introduced into this ammoniacal cupric solution, the free metallic copper dissolves in the ammonia set free by the fixation of the already dissolved copper upon and in the fibers of the cellulose in proportion as these dissolve.

The phenomena occurring in the operations described are of a physico-chemical nature, probably more ical. Thus, having knowledge of the dissolving action stated, it appears that it is not the ozone alone which acts, but there is a complex reaction resulting from the presence of ozone, alkali and cellulose, and causing nascent formations which in turn (2) The cotton is introduced into this ozo- I I physical than. chemcause p "cupric solution.

1. The process of making the cellulose to tating the solvent action of the ammoniacal Having thus described the nature of my said invention and the bestmeans I know of carrying the same into practical efiect,

a compound PlOdllCtlOIl of in subjecting ozone and an of cellulose adapted for the artificial silk, which consists the action of alkaline solution and formlng a solution of the cellulose thus treated.

2.; The process of I artificial silk, which consists in introducing the cellulose into an alkaline solution and yew-chemical plienbmeiai'tgilis.

making a compound- I of cellulose adapted for theyproductlon of nlily name this 5th day t passing throughn the mixture a; current' of ozone, and ma w.thustreated.

g a solution of the cellulose 3. The process oi making a, compound which consists in subjecting ozone and an In witness whereof I have hereunto signed of October 1906, in. e presence of two subscribing witnessw. 3Q

EMILE, CRUMIERE. Witnesses HANSON O. Cox'n. s GARBRIEL BELnIARn. I 

